Sperm oil fractionation



R. l. BRABETS ETAL SPERM OIL FRACTIONATION Filed DBG. l5, 1952 SPERMOILFRACTIONATION TOWER PRoPANe c GLYc amos INvsN-rofzs ATTORNEY nitedStates Patent ice 2,730,538 SPERM OIL FRACTIONATION Robert I. Brabets,Hazelcrest, and Robert J. Hlavacek,

Berwyn, Ill., and Earle Fritz, East Chicago, Ind., as-

signors to Swift & Company, Chicago, lll., a corporation of IllinoisApplication December 15, 1952, Serial No. 326,062 4 Claims. (Cl.260-409) The present invention relates in general to a new compositionof matter and to the method of producing the same, and more particularlyto a new liquid wax product and the method of obtaining the same fromsperm oil and derivatives thereof.

Spermaceti, which is important to the cosmetic industry, isconventionally recovered by seeding and pressing of crude sperm oil. YThis operation is expensive and results in the recovery of about 7%spermaceti based on the weight of the crude oil. Due to this costlyoperation which results in a relatively small yield, it is desirable toprovide an improved method for the recovery Yof spermaceti, or toprovide a new product capable of serving as a substitute for thespermaceti.

' It is therefore an object of the present invention to provide a newproduct which may be less expensive to prepare and which may beeiectively used as a substitute for spermaceti.

Another object of the present invention is to provide a method fortreating crude sperm oil or derivatives thereof to produce a new liquidwax product.

Additonal objects, if not specifically set forth herein, will be readilyapparent to one skilled in the art from the following detaileddescription of the invention:

The drawing represents a schematic illustration of a fractionating towerwhich may be used in carrying out the method of the present invention.

Generally, the present invention comprises the fractionation of spermoil or derivatives thereof with a liquefied, normally gaseoushydrocarbon under specific operating conditions to produce a materialwhich, after hydrogenation, may be used as a spermaceti substitute.

More specifically, it has been found that, by subjecting crude sperm oilor a derivative thereof, such as tout oil (a by-product from the hotpressing of crude sperm oil), to the action of a liqueed, normallygaseous hydrocarbon in the manner disclosed below, an overhead fractionis obtained which is extremely high in both saturated and unsaturatedwax content, and which contains a relatively small amount of glyceride.

Sperm oil is essentially composed of two types of chemical compounds.The triglyceride component constitutes .2S-30% of the crude oil whilethe remainder is made up of saturated and unsaturated wax esters, e. g.RCOOR.

2,730,538 Patented Jan. `10, 19.56

Spermaceti is a saturated wax ester of the above type, wherein R' and R"are at least C14 or longer. As aforesaid, only about 6-8% spermaceti canbe recovered from crudesperm oil. By the present method, an overheadfraction 10-30% of the total oil) is obtained which contains almostexclusively the Wax ester component of the oil, while the bottomfraction contains a reduced amount of wax ester and an increased amountof glyceride. The wax ester in the overhead fraction is a mixture ofboth saturates and unsaturates, and hence cannot be consideredspermaceti. However, by hydrogenation, this product may be utilized verysatisfactorily as a spermaceti substitute. It likewise nds considerablevalue, due to its low glyceride content, in the preparation ofglyceridefree calcium soaps for greases.

Referring now to the drawing, 10 designates a continuous, countercurrentfractionating tower of conventional design. The oil to be fractionated,i. e. sperm oil, tout oil or hydrogenated tout oil, is introduced intothe top of the tower through line 11. This material then passesdownwardly through the packed tower in contact with a rising column ofsolvent introduced into the tower through line l12. The solvent may beany of the known normally gaseous hydrocarbons heretofore used by theart in the fractionation of fatty materials, as for example ethane,propane, isobutane, or butane, or mixtures thereof. Preferably, propaneis employed as the solvent. The temperature and pressure conditionswithin the tower must be such as to maintain the solvent in the liquidphase. Although these conditions may vary considerably for somefractionations, it is esential in carrying out the present method thatthey be maintained within relatively narrow limits. The temperature mayrange from about 205 F. to about 215 F., although the preferredtemperature is about 210 F. The pressure within the tower may likewisevary within relatively narow limits, i. e. from about 600 p. s. i. toabout 700 p. s. i. Presures within the upper portion of this range areconsidered preferable. The solvent to oil ratio should be maintainedwithin the range of about 20:1 to 25:1. Under these conditions, theoverhead fraction, removed from the tower through line 13 will be foundto have a wax ester content of about 90% or better, while the bottomfraction removed through line 14 will be found to have a much smallerwax ester content and a correspondingly higher glyceride content. Thefollowing table illustrates typical runs at varying conditions withinthe specified ranges of operating conditions on sperm oil and tout oil,and clearly illustrates the results of such method. The data given isfor the purpose of illustration only, and is not to be construed asplacing any limitations on the scope of the present invention, otherthan those in the appended claims:

Table I Feedstock Operating Conditions Overhead Bottoms CompositionComposition Olliijgesliatton (percent) (percent) Temp., Press. R tiYield Yield Type F. (p. s. i.) a o (percent) (percent) Wax Glycer- WaxGlycer- Wax Glycer- Ester ide Ester 1de Ester ide 210- Crude Sperm Oil30 610 20:1 15 82 18 85 25 75 Tout Oil gli? 700 25:1 11 95 5 89 65 35 Do70 30 g1g- 700 25:1 55 92 8 57 43 The product, recovered from theoverhead fraction in the fractionation of sperm oil, is a liquid waxester fraction containing 10% glyceride or less. It is very light incolor (FAC 1), is somewhat less viscous than the starting material, hasan iodine value in the range of 55-65 and a free fatty acid content of1.0-l.5%. A small amount of spermaceti will crystallize from thefraction after prolonged standing at room temperature. When hydrogenatedin the usual manner, it may be used satisfactorily as a substitute forspermaceti in cosmetics.

Obviously, many modifications and variations of the invention ashereinbefore set forth may be made without departing from the spirit andscope thereof, and therefore only such limitations should be imposed asare indicated in the appended claims.

We claim:

l. A method for the production of a liquid wax product which comprises:subjecting an oil selected from the group consisting of crude .spermoil, tout oil and hydrogenated tout oil to the action of a liquefied,normally-gaseous hydrocarbon at a Atemperature within the range of 205F. to 215 F., a pressure within the range of 600 to 700 p. s. i., and ahydrocarbon to oil ratio within the range of 20:1 to 25:1; andseparating out a fraction of said oil by said treatment, said fractionhaving a high content of the wax ester component of said oil.

2. A method for the production of a liquid wax product which comprises:contacting an oil selected from the group consisting of crude `spermoil, tout oil and hydrogenated tout oil in a continuous, countercurrentfractionating zone with a liqueed, normally-gaseous hydrocarbon, thehydrocarbon to oil ratio ranging from 20:1 to 25:1; maintaining saidzone at a temperature of from 205 F. to 215 F. and at a pressure of from600 to 700 p. s. i.; and separating out an overhead fraction from saidzone, said fraction having a high content of the wax ester component ofsaid oil.

3. A method as in claim 2 wherein the liquefied, normally-gaseoushydrocarbon is propane.

4. A method of producing a substitute for spermaceti for use incosmetics which comprises subjecting a sperm oil to countercurrentextraction in the liquid phase with a normally gaseous liquidhydrocarbon at a temperature of from 20S-215 F., a pressure of from600-700 p. s. i., and a hydrocarbon to oil ratio of 20:1 to 25:1 wherebytwo phases are formed, one phase being relatively rich in wax esters andthe other phase relatively rich in glycerides, separating the phases andhydrogenating the phase rich in wax esters,

References Cited in the le of this patent UNITED STATES PATENTS2,077,837 Holwech Apr. 20, 1937 2,228,040 Voogt et a1 Ian. 7, 19412,505,338 Palmer Apr. 25, 1950 2,521,234 Leaders et al. Sept. 5, 1950

2. A METHOD FOR THE PRODUCTION OF A LIQUID WAX PRODUCT WHICH COMPRISES:CONTACTING AN OIL SELECTED FROM THE GROUP CONSISTING OF CRUDE SPERM OIL,TOUT OIL AND HYDROGENATED TOUT OIL IN A CONTINUOUS, COUNTERCURRENTFRACTIONATING ZONE WITH A LIQUEFIED, NORMALLY-GASEOUS HYDROCARBON, THEHYDROCARBON TO OIL RATIO RANGING FROM 20:1 TO 25:1; MAINTAINING SAIDZONE AT A TEMPERATURE OF FROM 205* F. TO 215* F. AND AT A PRESSURE OFFROM 600 TO 700 P. S. I.; AND SEPARATING OUT AN OVERHEAD FRACTION FROMSAID ZONE, SAID FRACTION HAVING A HIGH CONTENT OF THE WAX ESTERCOMPONENT OF SAID OIL.